CN116217255B - High-precision ceramic material for 5G signal base station and preparation method thereof - Google Patents

High-precision ceramic material for 5G signal base station and preparation method thereof Download PDF

Info

Publication number
CN116217255B
CN116217255B CN202310187511.8A CN202310187511A CN116217255B CN 116217255 B CN116217255 B CN 116217255B CN 202310187511 A CN202310187511 A CN 202310187511A CN 116217255 B CN116217255 B CN 116217255B
Authority
CN
China
Prior art keywords
parts
silicone resin
ceramic material
vinyl
signal base
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202310187511.8A
Other languages
Chinese (zh)
Other versions
CN116217255A (en
Inventor
李国文
何永东
何志远
袁桂余
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xinhua Shunda Electronic Ceramics Co ltd
Original Assignee
Xinhua Shunda Electronic Ceramics Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xinhua Shunda Electronic Ceramics Co ltd filed Critical Xinhua Shunda Electronic Ceramics Co ltd
Priority to CN202310187511.8A priority Critical patent/CN116217255B/en
Publication of CN116217255A publication Critical patent/CN116217255A/en
Application granted granted Critical
Publication of CN116217255B publication Critical patent/CN116217255B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • C04B35/78Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80Fibres, filaments, whiskers, platelets, or the like
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • C04B2235/3222Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/444Halide containing anions, e.g. bromide, iodate, chlorite
    • C04B2235/445Fluoride containing anions, e.g. fluosilicate
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52Constituents or additives characterised by their shapes
    • C04B2235/5276Whiskers, spindles, needles or pins
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562Heating rate
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567Treatment time
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74Physical characteristics
    • C04B2235/77Density
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74Physical characteristics
    • C04B2235/78Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02DCLIMATE CHANGE MITIGATION TECHNOLOGIES IN INFORMATION AND COMMUNICATION TECHNOLOGIES [ICT], I.E. INFORMATION AND COMMUNICATION TECHNOLOGIES AIMING AT THE REDUCTION OF THEIR OWN ENERGY USE
    • Y02D30/00Reducing energy consumption in communication networks
    • Y02D30/70Reducing energy consumption in communication networks in wireless communication networks

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention relates to the field of ceramic materials, in particular to a high-precision ceramic material for a 5G signal base station and a preparation method thereof, and the high-precision ceramic material comprises the following preparation raw materials in parts by weight: 90-95 parts of alpha-aluminum oxide, 6-8 parts of aluminum fluoride, 0.2-0.8 part of magnesium lanthanum aluminate, 3-5 parts of vinyl liquid silicone resin and 80-120 parts of organic solvent.

Description

High-precision ceramic material for 5G signal base station and preparation method thereof
Technical Field
The invention relates to the field of ceramic materials, in particular to a high-precision ceramic material for a 5G signal base station and a preparation method thereof.
Background
The 5G signal base station is core equipment of the 5G network, provides wireless coverage, realizes wireless signal transmission between a wired communication network and a wireless terminal, and needs a large amount of high-precision ceramic materials when the 5G signal base station is built, wherein the high-precision ceramic materials have strict requirements on the size, if the linear shrinkage rate is too large during production, internal stress can be generated in the high-precision ceramic materials, so that the precision is influenced by the size deformation, serious cracks are even generated, the requirement of the building specification of the 5G signal base station is not met, and the building progress of the 5G signal base station is delayed.
Disclosure of Invention
The invention aims to: aiming at the technical problems, the invention provides a high-precision ceramic material for a 5G signal base station and a preparation method thereof.
The technical scheme adopted is as follows:
the high-precision ceramic material for the 5G signal base station comprises the following preparation raw materials in parts by weight:
90-95 parts of alpha-alumina, 6-8 parts of aluminum fluoride, 0.2-0.8 part of magnesium lanthanum aluminate, 3-5 parts of vinyl liquid silicone resin and 80-120 parts of organic solvent.
Further, the preparation method comprises the following preparation raw materials in parts by weight:
95 parts of alpha-alumina, 8 parts of aluminum fluoride, 0.6 part of magnesium lanthanum aluminate, 5 parts of vinyl liquid silicone resin and 100 parts of organic solvent.
Further, the vinyl liquid silicone resin is a metal alkoxide modified vinyl liquid silicone resin.
Further, the preparation method of the metal alkoxide modified vinyl liquid silicone resin comprises the following steps:
mixing vinyl triethoxysilane and toluene, stirring uniformly, dripping dilute hydrochloric acid, heating to 40-50 ℃ after dripping, reacting for 8-12h, continuously heating to 85-95 ℃ for reacting for 1-3h, recovering room temperature, separating out an organic phase, concentrating under reduced pressure to obtain liquid vinyl silicone resin, dissolving the obtained liquid vinyl silicone resin with toluene under the protection of nitrogen, adding metal alkoxy compound, heating to 55-65 ℃ for reacting for 6-10h, and performing reduced pressure rotary evaporation.
Further, the metal alkoxide is a zirconium alkoxide.
Further, the zirconium alkoxy compound is tetra-n-propyl zirconate or tetra-isopropyl zirconate.
Further, the metal alkoxide is used in an amount of 5 to 12% by mass of the liquid vinyl silicone resin.
Further, the mass concentration of the dilute hydrochloric acid is 0.5-1%.
Further, the boiling point of the organic solvent is less than or equal to 100 ℃.
The invention also provides a preparation method of the high-precision ceramic material for the 5G signal base station, which comprises the following steps:
respectively drying alpha-alumina, aluminum fluoride and magnesium lanthanum aluminate, mixing to obtain first powder, diluting vinyl liquid silicone resin with an organic solvent, mixing with the first powder, ball milling, drying to remove the organic solvent to obtain second powder, compression molding the second powder to obtain a ceramic biscuit, heating and sintering the ceramic biscuit to 600-650 ℃ at first, heat-preserving and sintering for 90-120min, heating to 800-850 ℃ at second, heat-preserving and sintering for 90-120min, heating to 1400-1450 ℃ at third, heat-preserving and sintering for 120-180min, and finally cooling to room temperature along with a furnace.
The invention has the beneficial effects that:
the invention provides a high-precision ceramic material for 5G signal base station, the liquid silicone resin is a semi-inorganic semi-organic polymer with-Si-O-Si-as main chain, and can be cross-linked under a certain condition to form three-dimensional network structure product, and then the three-dimensional network structure product is mixed with alpha-alumina, aluminium fluoride and magnesium lanthanum aluminate, and the three-dimensional network structure can cover these ceramic powders into the ceramic material to form granules with a certain shape and strength, and in the course of sintering, the granules are decomposed and SiO is used 2 The form of/(Si-O-C-remains, forming alumina-SiO) 2 The aluminum fluoride ternary system generates mullite whiskers in situ during high-temperature sintering, the generated mullite whiskers are interpenetrated in the ceramic material to play a role of supporting and bridging, and the vinyl liquid silicon resin is oxidized and decomposed to generate gas during the high-temperature sintering process, the continuous overflow of the gas counteracts the internal stress generated by the internal densification of the ceramic material, the linear shrinkage rate is reduced, the production precision is improved, the inventor modifies the liquid silicon resin by using a metal alkoxy compound, metal elements are introduced into a high polymer chain after transesterification reaction, metal oxides can be formed to toughen and strengthen the ceramic material during sintering, and lanthanum magnesium aluminate can promote the sintering densification of the ceramic material, refine grains and improve the density and the mechanical strength.
Drawings
FIG. 1 is a diagram showing the microscopic morphology of a high-precision ceramic material according to example 1 of the present invention;
as can be seen from the figure, the mullite whisker is interpenetrated in the ceramic material to play a role of supporting and bridging.
Detailed Description
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention. The technology not mentioned in the present invention refers to the prior art.
Example 1:
the high-precision ceramic material for the 5G signal base station comprises the following preparation raw materials in parts by weight:
95 parts of alpha-alumina, 8 parts of aluminum fluoride, 0.6 part of magnesium lanthanum aluminate, 5 parts of vinyl liquid silicone resin and 100 parts of acetone.
Wherein the vinyl liquid silicone resin is tetra-n-propyl zirconate modified vinyl liquid silicone resin, and the preparation method comprises the following steps:
adding 1kg of vinyltriethoxysilane and 10L of toluene into a reaction kettle with a condenser, stirring to uniformly mix, dripping 285mL of diluted hydrochloric acid with the mass concentration of 1% into the reaction kettle by using a dropping funnel, heating to 45 ℃ after dripping, stirring and reacting for 10 hours, continuously heating to 95 ℃ and stirring and reacting for 2 hours, closing heating, naturally recovering room temperature, separating an organic phase, drying by using anhydrous sodium sulfate, decompressing and steaming to obtain liquid vinyl silicone resin, dissolving the obtained liquid vinyl silicone resin by using a proper amount of toluene under the protection of nitrogen, adding tetra-n-propyl zirconate with the mass of 10%, heating to 60 ℃ after reacting for 8 hours, transferring the reaction liquid to a rotary evaporator, decompressing and steaming.
The preparation method of the high-precision ceramic material for the 5G signal base station comprises the following steps:
drying alpha-aluminum oxide, aluminum fluoride and magnesium lanthanum aluminate at 100 ℃ for 10 hours respectively, mixing to obtain first powder, diluting the prepared tetra-n-propyl zirconate modified vinyl liquid silicone resin with acetone, mixing and ball milling with the first powder for 15 hours, drying at 85 ℃ for 24 hours, removing acetone to obtain second powder, transferring the second powder into a mould, carrying out compression molding under 15MPa pressure for 80 seconds to obtain a ceramic biscuit, heating and sintering the obtained ceramic biscuit in an air atmosphere, firstly heating to 650 ℃ at a speed of 10 ℃/min, carrying out heat preservation and sintering for 100 minutes, secondly heating to 820 ℃ at a speed of 5 ℃/min, carrying out heat preservation and sintering for 120 minutes, thirdly heating to 1430 ℃ at a speed of 2 ℃/min, carrying out heat preservation and sintering for 150 minutes, and finally cooling to room temperature along with a furnace.
Example 2:
the high-precision ceramic material for the 5G signal base station comprises the following preparation raw materials in parts by weight:
95 parts of alpha-alumina, 8 parts of aluminum fluoride, 0.8 part of magnesium lanthanum aluminate, 5 parts of vinyl liquid silicone resin and 120 parts of acetone.
Wherein the vinyl liquid silicone resin is tetra-n-propyl zirconate modified vinyl liquid silicone resin, and the preparation method is the same as that of the example 1;
the preparation method of the high-precision ceramic material for the 5G signal base station comprises the following steps:
drying alpha-aluminum oxide, aluminum fluoride and magnesium lanthanum aluminate at 100 ℃ for 10 hours respectively, mixing to obtain first powder, diluting the prepared tetra-n-propyl zirconate modified vinyl liquid silicone resin with acetone, mixing and ball milling with the first powder for 15 hours, drying at 85 ℃ for 24 hours, removing acetone to obtain second powder, transferring the second powder into a mould, carrying out compression molding under 15MPa pressure for 80 seconds to obtain a ceramic biscuit, heating and sintering the obtained ceramic biscuit in an air atmosphere, firstly heating to 650 ℃ at a speed of 10 ℃/min, carrying out heat preservation and sintering for 120 minutes, secondly heating to 850 ℃ at a speed of 5 ℃/min, carrying out heat preservation and sintering for 120 minutes, thirdly heating to 1450 ℃ at a speed of 2 ℃/min, carrying out heat preservation and sintering for 180 minutes, and finally cooling to room temperature along with a furnace.
Example 3:
the high-precision ceramic material for the 5G signal base station comprises the following preparation raw materials in parts by weight:
90 parts of alpha-alumina, 6 parts of aluminum fluoride, 0.2 part of magnesium lanthanum aluminate, 3 parts of vinyl liquid silicone resin and 80 parts of acetone.
Wherein the vinyl liquid silicone resin is tetra-n-propyl zirconate modified vinyl liquid silicone resin, and the preparation method is the same as that of the example 1;
the preparation method of the high-precision ceramic material for the 5G signal base station comprises the following steps:
drying alpha-aluminum oxide, aluminum fluoride and magnesium lanthanum aluminate at 100 ℃ for 10 hours respectively, mixing to obtain first powder, diluting the prepared tetra-n-propyl zirconate modified vinyl liquid silicone resin with acetone, mixing and ball milling with the first powder for 15 hours, drying at 85 ℃ for 24 hours, removing acetone to obtain second powder, transferring the second powder into a mould, carrying out compression molding under 15MPa pressure for 80 seconds to obtain a ceramic biscuit, heating and sintering the obtained ceramic biscuit in an air atmosphere, firstly heating to 600 ℃ at a speed of 10 ℃/min, carrying out heat preservation and sintering for 90 minutes, secondly heating to 800 ℃ at a speed of 5 ℃/min, carrying out heat preservation and sintering for 90 minutes, thirdly heating to 1400 ℃ at a speed of 2 ℃/min, carrying out heat preservation and sintering for 120 minutes, and finally cooling to room temperature along with a furnace.
Example 4:
the high-precision ceramic material for the 5G signal base station comprises the following preparation raw materials in parts by weight:
95 parts of alpha-alumina, 6 parts of aluminum fluoride, 0.8 part of magnesium lanthanum aluminate, 3 parts of vinyl liquid silicone resin and 120 parts of acetone.
Wherein the vinyl liquid silicone resin is tetra-n-propyl zirconate modified vinyl liquid silicone resin, and the preparation method is the same as that of the example 1;
the preparation method of the high-precision ceramic material for the 5G signal base station comprises the following steps:
drying alpha-aluminum oxide, aluminum fluoride and magnesium lanthanum aluminate at 100 ℃ for 10 hours respectively, mixing to obtain first powder, diluting the prepared tetra-n-propyl zirconate modified vinyl liquid silicone resin with acetone, mixing and ball milling with the first powder for 15 hours, drying at 85 ℃ for 24 hours, removing acetone to obtain second powder, transferring the second powder into a mould, carrying out compression molding under 15MPa pressure for 80 seconds to obtain a ceramic biscuit, heating and sintering the obtained ceramic biscuit in an air atmosphere, firstly heating to 600 ℃ at a speed of 10 ℃/min, carrying out heat preservation and sintering for 120 minutes, secondly heating to 800 ℃ at a speed of 5 ℃/min, carrying out heat preservation and sintering for 120 minutes, thirdly heating to 1400 ℃ at a speed of 2 ℃/min, carrying out heat preservation and sintering for 180 minutes, and finally cooling to room temperature along with a furnace.
Example 5:
the high-precision ceramic material for the 5G signal base station comprises the following preparation raw materials in parts by weight:
90 parts of alpha-alumina, 8 parts of aluminum fluoride, 0.2 part of magnesium lanthanum aluminate, 5 parts of vinyl liquid silicone resin and 80 parts of acetone.
Wherein the vinyl liquid silicone resin is tetra-n-propyl zirconate modified vinyl liquid silicone resin, and the preparation method is the same as that of the example 1;
the preparation method of the high-precision ceramic material for the 5G signal base station comprises the following steps:
drying alpha-aluminum oxide, aluminum fluoride and magnesium lanthanum aluminate at 100 ℃ for 10 hours respectively, mixing to obtain first powder, diluting the prepared tetra-n-propyl zirconate modified vinyl liquid silicone resin with acetone, mixing and ball milling with the first powder for 15 hours, drying at 85 ℃ for 24 hours, removing acetone to obtain second powder, transferring the second powder into a mould, carrying out compression molding under 15MPa pressure for 80 seconds to obtain a ceramic biscuit, heating and sintering the obtained ceramic biscuit in an air atmosphere, firstly heating to 650 ℃ at a speed of 10 ℃/min, carrying out heat preservation and sintering for 90 minutes, secondly heating to 850 ℃ at a speed of 5 ℃/min, carrying out heat preservation and sintering for 90 minutes, thirdly heating to 1450 ℃ at a speed of 2 ℃/min, carrying out heat preservation and sintering for 120 minutes, and finally cooling to room temperature along with a furnace.
Comparative example 1:
substantially the same as in example 1, except that lanthanum magnesium aluminate was not added.
Comparative example 2:
substantially the same as in example 1, except that the prepared tetra-n-propyl zirconate modified vinyl liquid silicone resin was replaced with a commercially available vinyl liquid silicone resin (delta DT-10050).
Performance test:
the ceramic materials prepared in examples 1 to 5 and comparative examples 1 to 2 of the present invention were used as test samples, the dimensions of the test samples before and after sintering were measured using a vernier caliper, the linear shrinkage was calculated, the flexural strength of the test samples was measured in units of a three-point bending method on a universal tester, the span was 30mm, the loading rate was 0.5mm/min, the fracture toughness of the test samples was measured and calculated in units of MPa.m using an indentation method 1/2 The test results are shown in Table 1 below:
table 1:
flexural Strength Fracture toughness Linear shrinkage rate
Example 1 166.2 3.05 0.36
Example 2 163.7 2.96 0.42
Example 3 159.3 2.84 0.44
Example 4 162.9 3.01 0.38
Example 5 165.5 3.03 0.37
Comparative example 1 130.4 2.16 0.38
Comparative example 2 126.8 2.01 1.03
As can be seen from the above Table 1, the ceramic material prepared by the invention has good mechanical properties and low linear shrinkage, and can meet the production requirements of high-precision ceramic materials.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (7)

1. The high-precision ceramic material for the 5G signal base station is characterized by comprising the following preparation raw materials in parts by weight:
90-95 parts of alpha-alumina, 6-8 parts of aluminum fluoride, 0.2-0.8 part of magnesium lanthanum aluminate, 3-5 parts of vinyl liquid silicone resin and 80-120 parts of organic solvent;
the vinyl liquid silicone resin is a metal alkoxide modified vinyl liquid silicone resin;
the preparation method of the metal alkoxide modified vinyl liquid silicone resin comprises the following steps:
mixing vinyl triethoxysilane and toluene, stirring uniformly, dripping dilute hydrochloric acid, heating to 40-50 ℃ after dripping, reacting for 8-12h, continuously heating to 85-95 ℃ for reacting for 1-3h, recovering room temperature, separating out an organic phase, concentrating under reduced pressure to obtain liquid vinyl silicone resin, dissolving the obtained liquid vinyl silicone resin with toluene under the protection of nitrogen, adding a metal alkoxy compound, heating to 55-65 ℃ for reacting for 6-10h, and concentrating under reduced pressure;
the metal alkoxide is a zirconium alkoxide.
2. The high-precision ceramic material for 5G signal base stations according to claim 1, comprising the following preparation raw materials in parts by weight:
95 parts of alpha-alumina, 8 parts of aluminum fluoride, 0.6 part of magnesium lanthanum aluminate, 5 parts of vinyl liquid silicone resin and 100 parts of organic solvent.
3. The high-precision ceramic material for 5G signal base stations according to claim 1, wherein the zirconium alkoxide compound is tetra-n-propyl zirconate or tetra-isopropyl zirconate.
4. The high-precision ceramic material for 5G signal base stations according to claim 1, wherein the metal alkoxide is used in an amount of 5 to 12% by mass of the liquid vinyl silicone resin.
5. The high-precision ceramic material for 5G signal base stations according to claim 1, wherein the mass concentration of the dilute hydrochloric acid is 0.5 to 1%.
6. The high-precision ceramic material for 5G signal base stations according to claim 1, wherein the boiling point of the organic solvent is 100 ℃.
7. The method for preparing the high-precision ceramic material for the 5G signal base station according to any one of claims 1 to 6, which is characterized in that alpha-alumina, aluminum fluoride and magnesium lanthanum aluminate are respectively dried and mixed to obtain first powder, vinyl liquid silicone resin is diluted by an organic solvent and then mixed with the first powder for ball milling, then the organic solvent is dried and removed to obtain second powder, the second powder is subjected to compression molding to obtain a ceramic biscuit, the ceramic biscuit is heated and sintered, the first stage is heated to 600 to 650 ℃, the heat is preserved and sintered for 90 to 120 minutes, the second stage is heated to 800 to 850 ℃, the heat is preserved and sintered for 90 to 120 minutes, the third stage is heated to 1400 to 1450 ℃, the heat is preserved and sintered for 120 to 180 minutes, and finally the ceramic biscuit is cooled to room temperature along with a furnace.
CN202310187511.8A 2023-03-02 2023-03-02 High-precision ceramic material for 5G signal base station and preparation method thereof Active CN116217255B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202310187511.8A CN116217255B (en) 2023-03-02 2023-03-02 High-precision ceramic material for 5G signal base station and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310187511.8A CN116217255B (en) 2023-03-02 2023-03-02 High-precision ceramic material for 5G signal base station and preparation method thereof

Publications (2)

Publication Number Publication Date
CN116217255A CN116217255A (en) 2023-06-06
CN116217255B true CN116217255B (en) 2023-12-15

Family

ID=86572770

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202310187511.8A Active CN116217255B (en) 2023-03-02 2023-03-02 High-precision ceramic material for 5G signal base station and preparation method thereof

Country Status (1)

Country Link
CN (1) CN116217255B (en)

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1304903A (en) * 2000-12-29 2001-07-25 清华大学 Process for preparing high-toughness alumina ceramics
CN102826837A (en) * 2012-09-12 2012-12-19 中国地质大学(北京) LaMgAl11O19-ZrO2-Al2O3 complex-phase wear-resistant ceramic material
CN104761243A (en) * 2015-03-26 2015-07-08 上海大学 Method for preparing ceramic core by combining thermosetting organic silicon resin with ceramic powder
CN105218101A (en) * 2015-11-11 2016-01-06 中国人民解放军国防科学技术大学 A kind of in-situ copolymerization polymer pyrolysis method preparing MC-SiC superhigh temperature ceramic material
CN106747541A (en) * 2016-12-05 2017-05-31 中南大学 A kind of method of the mullite ceramic of On In-situ Synthesis of Mullite Whisker self toughening
CN106747349A (en) * 2016-11-30 2017-05-31 上海大学 The method that in-situ preparation SiC strengthens alumina based ceramic core
CN107778006A (en) * 2016-08-29 2018-03-09 天津城建大学 High temperature resistant SiC zirconia ceramic aerogel heat-proof composite materials and its preparation method and application
CN108218407A (en) * 2018-01-24 2018-06-29 烟台金泰美林科技股份有限公司 A kind of valve alumina composite ceramic and preparation method thereof
WO2022001828A1 (en) * 2020-06-29 2022-01-06 比亚迪股份有限公司 Ceramic-like material, preparation method therefor, and application thereof

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1304903A (en) * 2000-12-29 2001-07-25 清华大学 Process for preparing high-toughness alumina ceramics
CN102826837A (en) * 2012-09-12 2012-12-19 中国地质大学(北京) LaMgAl11O19-ZrO2-Al2O3 complex-phase wear-resistant ceramic material
CN104761243A (en) * 2015-03-26 2015-07-08 上海大学 Method for preparing ceramic core by combining thermosetting organic silicon resin with ceramic powder
CN105218101A (en) * 2015-11-11 2016-01-06 中国人民解放军国防科学技术大学 A kind of in-situ copolymerization polymer pyrolysis method preparing MC-SiC superhigh temperature ceramic material
CN107778006A (en) * 2016-08-29 2018-03-09 天津城建大学 High temperature resistant SiC zirconia ceramic aerogel heat-proof composite materials and its preparation method and application
CN106747349A (en) * 2016-11-30 2017-05-31 上海大学 The method that in-situ preparation SiC strengthens alumina based ceramic core
CN106747541A (en) * 2016-12-05 2017-05-31 中南大学 A kind of method of the mullite ceramic of On In-situ Synthesis of Mullite Whisker self toughening
CN108218407A (en) * 2018-01-24 2018-06-29 烟台金泰美林科技股份有限公司 A kind of valve alumina composite ceramic and preparation method thereof
WO2022001828A1 (en) * 2020-06-29 2022-01-06 比亚迪股份有限公司 Ceramic-like material, preparation method therefor, and application thereof

Also Published As

Publication number Publication date
CN116217255A (en) 2023-06-06

Similar Documents

Publication Publication Date Title
CN106747541B (en) Method for in-situ synthesis of mullite whisker self-toughened mullite ceramic
CN108002822B (en) Silicon-aluminum hollow ball heat insulation product and preparation method thereof
CN115028460A (en) Preparation method of high-thermal-conductivity silicon nitride ceramic substrate
CN115594510A (en) Silicon nitride heat-conducting substrate and preparation method thereof
CN116217255B (en) High-precision ceramic material for 5G signal base station and preparation method thereof
CN113698201B (en) Composite zirconia powder, aluminum nitride ceramic substrate, and preparation method and application thereof
CN104108938A (en) Preparation method for Sialon ceramic
CN109796222A (en) The preparation method of beta-silicon nitride nanowire reinforcing silicon nitride foam ceramic
CN117164344A (en) Composite ceramic substrate and production process thereof
CN114853347A (en) High-thermal-conductivity low-temperature co-fired glass ceramic substrate and preparation method thereof
CN108178615B (en) Microwave ceramic dielectric sintered powder material, microwave dielectric ceramic and application thereof
CN106431419A (en) Preparation method of aluminum nitride ceramic substrate with high thermal conductivity for high power microelectronic devices
CN112266238B (en) Low dielectric constant ceramic material for microwave device and preparation method thereof
CN115286409A (en) Silicon nitride whisker reinforced aluminum nitride composite ceramic material and preparation method thereof
CN107793138A (en) A kind of aluminium oxide ceramics
CN113087501A (en) High-strength quartz ceramic roller and preparation process thereof
CN115304367A (en) Preparation method and product of microwave dielectric ceramic
CN110937902A (en) Preparation method of aluminum nitride ceramic substrate
CN112457047A (en) Preparation method of low-dielectric low-density quartz ceramic material
CN108503362B (en) Preparation method of nano graphite-based grinding material
JP4533994B2 (en) Plasma corrosion resistant material, manufacturing method thereof and member thereof
CN112707721A (en) Silicon carbide toughened microwave dielectric ceramic material and preparation method thereof
CN114149273B (en) Preparation method of alumina ceramic powder for electronic ceramics
CN109721381A (en) The preparation method of silicon nitride shell reinforcing silicon nitride foam ceramic
CN115710129B (en) Preparation method of silicon nitride ceramic

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant